CN2856060Y - High vacuum in-situ refining equipment extracting high pure material - Google Patents
High vacuum in-situ refining equipment extracting high pure material Download PDFInfo
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- CN2856060Y CN2856060Y CNU2005201273638U CN200520127363U CN2856060Y CN 2856060 Y CN2856060 Y CN 2856060Y CN U2005201273638 U CNU2005201273638 U CN U2005201273638U CN 200520127363 U CN200520127363 U CN 200520127363U CN 2856060 Y CN2856060 Y CN 2856060Y
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The utility model discloses a high vacuum home position refining apparatus for abstracting high purity and ultra-pure materials. The high vacuum refining apparatus comprises an abstracting cavity, a vacuum system, a diffusion furnace, a crucible, a feeding/retrieving system, a protective gas device and an industrial intelligent temperature controller and the each part is connected via vacuum pipe fittings, gas paths and conducting wires to form a refining apparatus integration. With regard to its prominent advantages, the apparatus can respectively and effectively eliminate the highly saturated steam pressure impurities and low saturated steam pressure impurities by stages. The abstracting process is kept in a high vacuum state consistently and the production process as a whole is isolated from the atmosphere. The contamination to the raw materials caused by the atmosphere is greatly reduced. The apparatus produces high quality products with powerful production capability. The apparatus is stable and reliable in terms of the performance thereof, suitable for producing high purity and ultra-pure materials, in particular for the preparation of highly active high purity materials.
Description
Technical field
The utility model relates to a kind of high-vacuum in-situ refining apparatus of producing high-purity and ultra-pure material, belongs to high-purity and ultra-pure material field of smelting in metallurgical and the chemical industry.
Background technology
High-purity material such as high pure metal, high-purity nonmetal and high-purity inorganic compound-material etc. have a wide range of applications at preparation compound semiconductor materials and fields such as device and Aeronautics and Astronautics, as metals such as the zinc that uses in II-VI, the III-V compound semiconductor, magnesium, calcium, aluminium, arsenic, phosphorus and its purity requirement of non-metallic material more than 99.999% (5N), otherwise too much impurity can have a strong impact on the crystallinity and the photoelectric characteristic of semiconductor material, thereby device performance is descended greatly.At present, vacuum distilling method or zone melting method etc. are adopted in the production of high pure metal more, as Chinese patent 98113973.6,200320115091.0,200320115092.5 and foreign patent KR2004022842-A, RU2236476-C1, the refining equipment and the method for JP10121163-A etc. report, when metal is in high temperature, its vacuum tightness generally at 10 handkerchiefs between 0.01 handkerchief, residual gas in the vacuum chamber is also quite a lot of, and this refinement for the active metal is quite harmful; In addition, very big to the separation and the removal effect difference of different impurities in the refining hihg purity metal process, lack the efficient simultaneously method of removing high saturated vapor pressure and low saturated vapor pressure impurity, thereby influence total refining effect.Wet process technique is generally adopted in the production of high pure metal at present, and is big to environmental hazard, simultaneously unstable product quality.In addition, adopt reaction method to make more, still lack the means of purifying efficiently some mineral compound materials.
The utility model content
The purpose of this utility model is the high-vacuum in-situ refining apparatus that a kind of brand-new extracting high-purity material is provided at the deficiencies in the prior art, can improve refining effect greatly, not only steady quality is reliable, and the refinement technique of environment amenable high-purity material and equipment have important industrial application value.
For achieving the above object, a kind of high-vacuum in-situ refining apparatus that is used for extracting high-purity material of the utility model comprises: material system, shielding gas device and industrial intelligent temperature regulator (abbreviation temperature controller) are got in vacuum system, refinement chamber, diffusion furnace, crucible, charging; Charging is got the material system and is linked to each other with the refinement chamber, diffusion furnace is installed in and refines the bottom, chamber, crucible is arranged in the diffusion furnace, temperature controller links to each other with diffusion furnace by thermocouple compensation wire and lead, vacuum system links to each other with the shielding gas device with diffusion furnace respectively, is provided with two independently heater strips in the diffusion furnace, i.e. top heater strip and lower heating silk, can heat the top and the bottom of crucible respectively, to form the low or upward low high temperature distribution of relative superiority or inferiority; A crucible cover also is installed, uniform distribution aperture on the crucible cover on the mouth of described crucible.
Further, described vacuum system comprises forepump, molecular pump, ionic pump and vacuum measurement instrument, molecular pump links to each other with forepump, and described forepump comprises mechanical pump or dried pump equal vacuum pump, and Pirani gauge and ion gauge or compound gauge are installed between described forepump and the molecular pump.
Further, described refinement chamber is divided into two portions up and down, connects by a slide valve, refines top, chamber and is connected by another slide valve with described molecular pump, refines the bottom, chamber and links to each other with described ionic pump, refines top, chamber ion gauge or compound gauge also are installed.
Further, the material system is got in described charging, and the shift fork, magnetic force hand, quick feeding valve, viewing window, the cavity wall that refine top, chamber are linked up with and the transparent sealing case is formed by being installed in, and the transparent sealing case links to each other with top, described refinement chamber.
Further, described shielding gas device comprises gas cylinder, reducing valve, gas circuit and leaks valve, and the shielding gas device joins with the inlet mouth and the transparent sealing case inlet mouth of described molecular pump respectively.
Further, a condensation baffle plate that is used to collect high saturated vapor pressure impurity is also installed on top, described refinement chamber.
Further, handle is equipped with on the top of described crucible, can cooperate with described shift fork crucible is taken out in diffusion furnace, and move to refinement top, chamber, is taken out by the charging valve again.
The utility model utilizes two heater strip diffusion furnaces independently to control the temperature of crucible top and bottom, on different steps forms relative superiority or inferiority low and on low high temperature distribution, two-step approach is removed high saturated vapor pressure and low saturated vapor pressure impurity respectively under high vacuum condition, the first step: crucible is removed high saturated vapor pressure impurity according to the low temperature distribution temperature-gradient method of last relative superiority or inferiority, second step: crucible forms low high temperature distribution, temperature of lower is risen to vertex keep the some time, allow the raw materials evaporate that is in the bottom, near and lower local crystallization or the condensation of the temperature crucible mouth, the purification material is separated with low saturated vapor pressure impurity, thereby obtain high-purity material.In addition, the utility model also has following advantage:
1, the utility model high-vacuum in-situ refining apparatus is connected fully and isolated from atmosphere with the tight of refinement chamber by watertight chest, whole process of production is all carried out under shielding gas, simultaneously according to material characteristics, can select shielding gas flexibly for use, thereby greatly reduce in the air multiple composition the pollution of high-purity material;
2, when refining material, whole refinement chamber keeps high vacuum state, and background air pressure is 1 * 10
-4Below the handkerchief; During charging, refine top, chamber and fill shielding gas, but refining bottom, chamber and top separates by slide valve, and utilize ionic pump to bleed, still keep high vacuum state, thereby reduced the reaction that is in pyritous high-purity material and residual gas when refining and compound effectively, reduced the influence of gas widely, be particularly suitable for the purification of active material material;
3, during production, the staff isolates fully with the refinement material, and labor condition is good; The poisonous steam that produces during refinement can or be collected in the condensation baffle plate by the vacuum system discharging, pollutes little;
4, the utility model apparatus structure is simple, and firm and durable is simple to operate, convenient, constant product quality;
5, the utility model is fit to by many series combinations of transparent sealing case very much, and forms streamline, the production efficiency height, and output is big.
Description of drawings
Fig. 1 is used for the block diagram of the high-vacuum in-situ refining apparatus of extracting high-purity material for the utility model.
1 refines the chamber, 2 vacuum systems, and 3 diffusion furnaces, 4 crucibles, the material system is got in 5 chargings, 6 shielding gas devices, 7 temperature controllers.
Fig. 2 is the utility model high-vacuum in-situ refining apparatus agent structure synoptic diagram.
8 refine top, chamber, and 9 refine the bottom, chamber, 10,41 slide valves, 11 transparent sealing chambeies, 3 diffusion furnaces, 4 crucibles, 7 temperature controllers, 12 molecular pumps, 13 forepumps, 14 ionic pumps, 15 ion gauges or compound gauge, 16 Pirani gauges, 17 protection gas cylinders, 18 condensation baffle plates.
Fig. 3 gets material system architecture synoptic diagram for charging.
11 transparent sealing casees, 19 quick feeding valves, 20 shift forks, 21 magnetic force hands, 22 viewing windows, 23 cavity walls hook, 4 crucibles, 24 glove ports.
Fig. 4 is for being used for the special diffusion furnace structural representation of extracting high-purity material in the utility model.
25 body of heater shells, 26 radioprotective metallic cylinder, 27PBN insulating support, 28 top heater strips, 29 lower heating silks, 30 top thermocouples, 31 bottom thermocouples, 32 multilayer radioprotective tinsels, 33 vacuum flanges, 34 thermocouple joints, 35 power connections.
Fig. 5 is for being used for the crucible structural representation of extracting high-purity material in the utility model.
36 crucible main bodys, 37 crucible covers, 38 crucibles hook.
Embodiment
Below in conjunction with embodiment and accompanying drawing the utility model is elaborated, but can not be interpreted as restriction the utility model protection domain.
The block diagram of the utility model high-vacuum in-situ refining apparatus as shown in Figure 1, this device comprises: material system 5, shielding gas device 6 and industrial intelligent temperature regulator (abbreviation temperature controller) 7 got in refinement chamber 1, vacuum system 2, diffusion furnace 3, crucible 4, charging.Vacuum system 2 transversely links to each other with refinement chamber 1, and shielding gas device 6 links to each other with vacuum system 2 by valve; And diffusion furnace 3 and charging are got material system 5 and are connected with the bottom and the top of refining chamber 1 respectively along the longitudinal, and temperature controller 7 passes through the thermocouple compensation wire and power lead links to each other with diffusion furnace 3.
The utility model high-vacuum in-situ refining apparatus agent structure synoptic diagram as shown in Figure 2 wherein refines chamber 1 by refining top, chamber 8 and refining bottom, chamber 9 and form, and they connect by slide valve 10; Refine top, chamber 8 and be connected, refine bottom, chamber 9 and be connected, and diffusion furnace 3 links to each other with temperature controller 7 by thermocouple compensation wire and power lead with diffusion furnace 3 with transparent sealing case 11.Vacuum system 2 is by molecular pump 12, and forepump 13, ionic pump 14, ion gauge 15 and Pirani gauge 16 are formed.Molecular pump 12 is connected with refinement top, chamber 8 by a slide valve 41, and molecular pump 12 is connected with protection gas cylinder 17 by leakage valve, relief valve again.Ionic pump 14 is connected with refinement bottom, chamber 9 by a slide valve 10.Slide valve 10 tops are also installed a condensation baffle plate 18 and are used for the various steam that condensation diffuses out from the crucible mouth, and are replaceable, practical and convenient.
Material system architecture synoptic diagram is got in charging as shown in Figure 3, and this system is made up of transparent sealing case 11, quick feeding valve 19, shift fork 20, magnetic force hand 21, viewing window 22, cavity wall hook 23 and crucible 4.During charging, at first in the transparent sealing case, an amount of raw material packed in the crucible, crucible 4 is hung on the hook 23 of cavity wall then, cover charging valve 19 completely.Pumping high vacuum is opened then and is refined chamber 1 slide valve 10, utilizes shift fork 20 that crucible 4 is put into diffusion furnace 3.And when getting material, utilize shift fork 20 that crucible is taken out from diffusion furnace 3, and hang on the hook 23; Close slide valve 10, stop molecular pump 12, mechanical pump fills protection gas, opens charging valve 19, takes out crucible 4 and puts to transparent sealing case 11; Then material is taken out from crucible 4, choose the intermediary recrystallize and partly take a sample, detect, qualified product are encapsulated.There is glove port 24 transparent sealing case 11 both sides, and relating operation is undertaken by gloves 24, and in the whole process of production, high-purity material and atmosphere separate, and guarantee stable and reliable product quality; Simultaneously, the staff isolates fully with the refinement material, and working condition is good.
Be illustrated in figure 4 as the diffusion furnace structural representation of extracting high-purity material, it is characterized in that on PBN insulating support 27, being wound with upper and lower two-layer independent heater strip, be top heater strip 28 and lower heating silk 29, can realize independent control to crucible 4 upper and lower part temperature, on different steps forms relative superiority or inferiority low and on low high temperature distribution.Two-step approach is refined material under high vacuum condition, thereby removes high saturated vapor pressure and low saturated vapor pressure impurity respectively, the first step: crucible 4 is removed high saturated vapor pressure impurity according to the low temperature distribution temperature-gradient method of last relative superiority or inferiority; High saturated vapor pressure impurity evaporates then from raw material discharges from the aperture of crucible cover, condenses on the condensation baffle plate or by vacuum system and takes away; The purpose that crucible 4 upper temps are high is to stop impurity steam to condense on top.Second step: crucible 4 forms goes up low high temperature distribution, temperature of lower is risen to vertex keep the some time, allow the raw materials evaporate that is in the bottom, and near 4 mouthfuls of crucibles the lower local recrystallize of temperature, the purification material is separated with low saturated vapor pressure impurity, reach the purpose of extracting high-purity material.As shown in Figure 4, other parts of stove are body of heater shell 25, multilayer radioprotective metallic cylinder 26, top thermocouple 30, bottom thermocouple 31, multilayer radioprotective tinsel 32, vacuum flange 33, thermocouple joint 34, power connection 35; Wherein body of heater shell 25, radioprotective metallic cylinder 26, heater strip are high-purity refractory material as being not less than 99.99% High-purity Tantalum, niobium, molybdenum etc., and it is at high temperature pollution-free to guarantee to be refined starting material.
Be illustrated in figure 5 as the structural representation of crucible, it is characterized in that on 36 mouthfuls of the crucible main bodys crucible cover 37 being arranged, can with the crucible tight joint, it is that aperture about 1mm is used for discharging high saturated vapor pressure impurity that equally distributed aperture is arranged on the crucible cover.Load onto the quantity proper raw material and make that raw material integral body all is positioned at the zone that the lower furnace heater strip is controlled when refining in crucible, just ingredient upper surface is not higher than the upper end of lower heating silk.Behind the charged, cover crucible cover 37; Hook 38 is arranged at crucible main body top, can cooperate mobile crucible with shift fork, carries out charging and the operation of getting material.The crucible main body adopts materials such as high-purity PBN, high purity quartz or high-purity ceramic to make, crucible cover, the hook high-purity refractory material of employing such as High-purity Tantalum, niobium, molybdenum, PBN, quartz, high-purity corundum pottery etc. are made, thereby it is at high temperature pollution-free to guarantee to be refined starting material.
We utilize the inductively coupled plasma emission spectrometer preceding to refining, once refine and the purity of the MAGNESIUM METAL of secondary after refining and the major impurity that is comprised such as high saturated vapor pressure zinc impurities, low saturated vapor pressure impurity silicon and iron are tested, its result is as shown in table 1; The result shows that the purity of utilizing the utility model high-vacuum in-situ refining apparatus once to refine the back MAGNESIUM METAL reaches more than 99.995%, and the purity of secondary after refining reaches the demand of most advanced and sophisticated industries such as satisfying semiconductor material and device, aerospace more than 99.9992% fully, has very big economic benefit and social benefit.
Analysis before purity that table 1 the utility model once refines, secondary refines the high-purity magnesium of gained and contained major impurity and the refinement relatively
| Refine number of times | The content of major impurity (ppm) in the MAGNESIUM METAL | The purity of magnesium (%) | ||
| Zinc (Zn) | Silicon (Si) | Iron (Fe) | Magnesium (Mg) | |
| Refine and once refine the secondary refinement | 53 0.9 0.2 | 47 8.2 1.9 | 35 1.4 0.2 | 99.95％ ≥99.995％ ≥99.9992％ |
Claims (7)
1, a kind of high-vacuum in-situ refining apparatus that is used for extracting high-purity material is characterized in that, this device comprises: material system, shielding gas device and industrial intelligent temperature regulator are got in vacuum system, refinement chamber, diffusion furnace, crucible, charging; Charging is got the material system and is linked to each other with the refinement chamber, diffusion furnace is installed in and refines the bottom, chamber, crucible is arranged in the diffusion furnace, temperature controller links to each other with diffusion furnace by thermocouple compensation wire and lead, vacuum system links to each other with the shielding gas device with diffusion furnace respectively, is provided with two independently heater strips in the diffusion furnace, i.e. top heater strip and lower heating silk, can heat the top and the bottom of crucible respectively, to form the low or upward low high temperature distribution of relative superiority or inferiority; A crucible cover also is installed, uniform distribution aperture on the crucible cover on the mouth of described crucible.
2, a kind of high-vacuum in-situ refining apparatus that is used for extracting high-purity material according to claim 1, it is characterized in that, described vacuum system comprises forepump, molecular pump, ionic pump and vacuum measurement instrument, molecular pump links to each other with forepump, described forepump comprises mechanical pump or dried pump equal vacuum pump, and Pirani gauge and ion gauge or compound gauge are installed between described forepump and the molecular pump.
3, a kind of high-vacuum in-situ refining apparatus that is used for extracting high-purity material according to claim 2, it is characterized in that, described refinement chamber is two portions up and down, connect by a slide valve, refining top, chamber is connected by another slide valve with described molecular pump, refine the bottom, chamber and link to each other, refine top, chamber ion gauge or compound gauge also are installed with described ionic pump.
4, a kind of high-vacuum in-situ refining apparatus that is used for extracting high-purity material according to claim 3, it is characterized in that, the material system is got in described charging, and the shift fork, magnetic force hand, quick feeding valve, viewing window, the cavity wall that refine top, chamber are linked up with and the transparent sealing case is formed by being installed in, and the transparent sealing case links to each other with top, described refinement chamber.
5, a kind of high-vacuum in-situ refining apparatus that is used for extracting high-purity material according to claim 4; it is characterized in that; described shielding gas device comprises gas cylinder, reducing valve, gas circuit and leaks valve, and the shielding gas device joins with the inlet mouth and the transparent sealing case inlet mouth of described molecular pump respectively.
6, a kind of high-vacuum in-situ refining apparatus that is used for extracting high-purity material according to claim 5 is characterized in that, a condensation baffle plate that is used to collect high saturated vapor pressure impurity is also installed on top, described refinement chamber.
7, according to the described a kind of high-vacuum in-situ refining apparatus that is used for extracting high-purity material of claim 6, it is characterized in that handle is equipped with on the top of described crucible, can cooperate with described shift fork crucible is taken out in diffusion furnace, and move to refinement top, chamber, take out by the charging valve again.
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| Application Number | Priority Date | Filing Date | Title |
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| CNU2005201273638U CN2856060Y (en) | 2005-10-11 | 2005-10-11 | High vacuum in-situ refining equipment extracting high pure material |
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| CNU2005201273638U CN2856060Y (en) | 2005-10-11 | 2005-10-11 | High vacuum in-situ refining equipment extracting high pure material |
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| CN2856060Y true CN2856060Y (en) | 2007-01-10 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104588622A (en) * | 2014-12-24 | 2015-05-06 | 北方民族大学 | Metal melt bulk nanometer material preparing system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104588622A (en) * | 2014-12-24 | 2015-05-06 | 北方民族大学 | Metal melt bulk nanometer material preparing system |
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Legal Events
| Date | Code | Title | Description |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20070110 Termination date: 20091111 |